CN112142032A - Porous charcoal containing three-dimensional amorphous carbon framework and preparation method and application thereof - Google Patents
Porous charcoal containing three-dimensional amorphous carbon framework and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides porous charcoal containing a three-dimensional amorphous carbon framework and a preparation method and application thereof, wherein the preparation method comprises the following steps: pretreatment: preparing dry wood into a wood block, dissolving out part of components in the wood block through a solvent, and enriching a micro-nano pore structure of the wood block to form a porous wood block; stabilizing the pore structure: washing the porous wood block for several times by using deionized water, and then freeze-drying; amorphous carbon formation: and pyrolyzing the freeze-dried porous wood block through double temperature gradients to obtain the porous charcoal containing the three-dimensional amorphous carbon framework and modified by the nano particles. The preparation method has simple preparation conditions; the prepared porous charcoal containing the three-dimensional amorphous carbon frame has excellent comprehensive wave-absorbing effect, can be used as a wave-absorbing material, and provides a new way for value-added efficient utilization of forest biomass.
Description
Technical Field
The invention belongs to the field of intersection of wave-absorbing material technology and wood technology, and particularly relates to porous charcoal containing a three-dimensional amorphous carbon frame, a preparation method of the porous charcoal and application of the porous charcoal containing the three-dimensional amorphous carbon frame as a wave-absorbing material.
Background
The electromagnetic technology promotes the rapid development of society, and brings serious threats to the physical and mental health of human beings, the operation of electronic equipment and the invisibility of weaponry. Therefore, how to efficiently absorb the polluted electromagnetic waves is widely regarded and researched in the civil and military fields. Besides the strong absorption capacity, the excellent wave-absorbing material also has the characteristics of light weight and wide effective absorption frequency band, and is an important development trend in the field of the wave-absorbing material at present.
In recent years, new carbon materials (such as graphene and carbon nanotubes) have been widely used in the field of wave-absorbing materials by researchers due to their characteristics of good stability, low density, large specific surface area, high electrical conductivity, and the like. However, due to excessive electrical loss and no magnetic loss, it is difficult to obtain ideal impedance matching conditions and weak electromagnetic wave absorption capability, and it is difficult to meet the requirements of high strength, wide frequency and light weight. In addition, the raw materials (fossil) of the materials are high in cost, the preparation process is complex and energy consumption is high, and further expansion and application of the materials are greatly restricted. Forest biomass is a natural renewable resource, has the advantages of cost, environment and carbon content, and also has highly ordered nutrient delivery three-dimensional hollow microtubes which are difficult to realize by conventional chemical synthesis, and have regular pipelines and high porosity. When electromagnetic waves are injected along the hollow pipeline, most of the incident waves can be subjected to multiple scattering and dielectric attenuation in the micro pipeline, and radiation or interference of the electromagnetic waves can be effectively reduced. In addition, elements such as nitrogen, phosphorus, iron, oxygen and the like reserved in the porous charcoal can optimize dielectric loss and improve impedance matching level, so that the electromagnetic wave absorption capacity is enhanced.
However, at present, the research of applying the forest biomass porous carbon material to the field of wave-absorbing materials is few, and the comprehensive wave-absorbing effect is not ideal.
Disclosure of Invention
In view of the above technical problems in the prior art, an object of the present invention is to provide a method for preparing porous charcoal containing a three-dimensional amorphous carbon framework, wherein the porous charcoal prepared by the method has a natural three-dimensional ordered pore structure of wood and simultaneously introduces nanopores and nanoparticles, such that the prepared porous charcoal has an excellent comprehensive wave-absorbing effect at a low filling degree.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a preparation method of porous charcoal containing a three-dimensional amorphous carbon framework comprises the following steps:
s1, preprocessing: preparing dry wood into a wood block, dissolving out part of components in the wood block through a solvent, and enriching a micro-nano pore structure of the wood block to form a porous wood block;
s2, stable pore structure: washing the porous wood block for several times by using deionized water, and then freeze-drying;
s3, amorphous carbon: and (4) pyrolyzing the porous wood block treated in the step S2 through double temperature gradients to obtain the nanoparticle-modified porous charcoal containing the three-dimensional amorphous carbon framework.
The manner in which the dried wood is made into wood blocks may include any manner disclosed in the prior art, including but not limited to sawing, cutting, etc.
In some embodiments, the porous charcoal containing the three-dimensional amorphous carbon framework has a micron-nanometer graded porous structure, the specific surface area is more than 300 square meters per gram, and the density is less than 0.25g/cm3。
In some embodiments, in step S1, the solvent is an acidic sodium chlorite solution or a mixed solution of sodium hydroxide and sodium sulfite.
In some embodiments, in order to avoid the dissolution reaction to destroy the natural three-dimensional ordered pore structure of the wood block (such as the problems of cracking and collapse of hollow microtubes), the mass fraction of the acidic sodium chlorite solution is 1-10%, and the pH value of the solution is 2-4; preferably, the acid in the solution is one or a mixture of more than two of hydrochloric acid, glacial acetic acid and sulfuric acid; the temperature of the wood block in the acidic sodium chlorite solution is 20-100 ℃, and the reaction time is 1-12 h; preferably, the reaction temperature in the acidic sodium chlorite solution is 60-100 ℃, and the reaction time is 4-7 h.
In some embodiments, the ratio of the mass of the wood block to the volume of the acidic sodium chlorite solution is (1-3) g:50mL in order to allow for adequate dissolution of some of the components from the wood block and to ensure that hollow microtubes of the wood block do not suffer damage.
In some embodiments, the reaction temperature of the wood block in the mixed solution is 100-140 ℃, and the reaction time is 1-12h, wherein the mixed solution is a mixed solution of sodium hydroxide and sodium sulfite; preferably, the reaction time is 3 to 7 hours.
In some embodiments, the ratio of the mass of the wood piece to the volume of the mixed solution is (1-5) g:50 mL.
In some embodiments, in the step S3, the first temperature of the pyrolysis is 180-; the second temperature is 500-750 ℃, the heat preservation is carried out for 1-3h, a tube furnace and a muffle furnace filled with inert protective atmosphere can be adopted, and the carbon-containing components in the wood can be converted into amorphous carbon with weak conductivity by adopting the gradient temperature.
In some embodiments, in step S2, freeze-drying is performed to ensure that the three-dimensional ordered hollow microtubes and nanopore structures in the wood block do not undergo changes such as collapse and shrinkage during the drying process, and preferably the drying temperature is (-40) - (-80) deg.c, and the drying time is 48-60 h.
Another object of the present invention is to provide a porous charcoal containing a three-dimensional amorphous carbon framework, which is prepared by the method for preparing a porous charcoal containing a three-dimensional amorphous carbon framework according to any one of the above embodiments.
The invention also aims to provide a wave-absorbing material prepared from the porous charcoal containing the three-dimensional amorphous carbon framework.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, while a three-dimensional ordered hollow micro-tube structure of wood is utilized, a micron nanometer hierarchical porous structure is formed in a wood block by means of partial dissolution of components in the wood, so that a porous wood block with a large specific surface area is obtained; then, removing chemical agents in the wood by deionized water cleaning, and adopting freeze drying to ensure that the micro-nano pore structure does not have the problems of collapse, shrinkage and the like in the drying process and stabilize the three-dimensional pore structure; and finally, pyrolyzing the freeze-dried porous wood block at a first temperature through dual-temperature gradient pyrolysis to further stabilize the three-dimensional micro-nano pore structure and promote the formation of nano particles, and then pyrolyzing at a second temperature to change carbon-containing components in the wood into amorphous carbon with weak conductivity.
The preparation method provided by the invention has the advantages of simple preparation process and low cost, and is beneficial to industrial production.
The porous charcoal containing the three-dimensional amorphous carbon frame prepared by the preparation method provided by the invention has the characteristics of large specific surface area, moderate conductivity and good impedance matching property, compared with the traditional carbon-based wave-absorbing material, the preparation method is simple in process and low in cost, has the advantages of high absorption strength under low filling degree, wide effective absorption frequency band and the like, has excellent wave-absorbing property, has a wide application prospect in the field of wave-absorbing materials, and can be used as the wave-absorbing material. The invention provides a new way for value-added efficient utilization of forest biomass.
Drawings
FIG. 1 is a flow chart of a production process of the present invention;
FIG. 2 is an XRD spectrum of porous charcoal containing a three-dimensional amorphous carbon framework prepared in example 1 of the present invention;
FIG. 3 is an SEM image of porous charcoal containing a three-dimensional amorphous carbon framework prepared in example 1 of the present invention;
fig. 4 is a graph showing reflection loss of porous charcoal containing a three-dimensional amorphous carbon framework prepared in example 1 of the present invention.
Detailed Description
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein, but rather should be construed as broadly as the present invention is capable of modification in various respects, all without departing from the spirit and scope of the present invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
Example 1
As shown in fig. 1, a preparation method of porous charcoal containing a three-dimensional amorphous carbon framework comprises the following steps:
s1, preprocessing: sawing native wood (taking masson pine as an example, air-dried or oven-dried) into wood blocks with the thickness of 10mm, putting the wood blocks into 500mL of acidic sodium chlorite solution with the mass fraction of 2%, treating for 6-7h at the temperature of 60-75 ℃, dissolving out part of components in the wood blocks, enriching micro-nano pore structures of the wood blocks, and forming porous wood blocks; wherein the pH value of the solution is 2, and the ratio of the mass of the wood block to the volume of the solution is 3g:50 mL;
s2, stable pore structure: washing the porous wood block for several times by using deionized water to remove residual chemical agents; then freeze-drying at-50 deg.C for 50 h;
s3, amorphous carbon: and (4) putting the porous wood block dried in the step S2 into a tubular furnace filled with inert gas, heating to 250 ℃ and preserving heat for 2 hours, heating to 650 ℃ and preserving heat for 3 hours, and cooling to room temperature to obtain the nanoparticle modified porous charcoal containing the three-dimensional amorphous carbon framework.
The porous charcoal containing the three-dimensional amorphous carbon framework prepared in the example is characterized by XRD and SEM respectively, and an XRD analysis chart is shown in figure 2, and an SEM analysis chart is shown in figure 3.
As shown in figure 3, the porous charcoal containing the three-dimensional amorphous carbon frame prepared in the embodiment has high specific surface area which is more than 300 square meters per gram and has the density which is less than 0.25g/cm through testing3(ii) a The average pore diameter of the three-dimensional amorphous carbon framework is about 20 mu m, and the filling degree of nano particles in the three-dimensional amorphous carbon framework is low。
The porous charcoal containing the three-dimensional amorphous carbon frame prepared in the embodiment is pressed into concentric rings with the outer diameter of 7mm and the inner diameter of 3.04mm, and an electromagnetic performance test is performed, wherein the reflection loss performance at different thicknesses is shown in fig. 4.
As shown in fig. 4, the reflection loss of the porous charcoal containing the three-dimensional amorphous carbon frame prepared in this example is below-30 dB, wherein when the thickness is 2.5mm, the wave-absorbing performance is significant, and the optimal reflection loss reaches-64 dB.
Example 2
A preparation method of porous charcoal containing a three-dimensional amorphous carbon framework comprises the following steps:
s1, preprocessing: sawing the primary wood (air-dried or oven-dried) into wood blocks with the thickness of 7mm, putting the wood blocks into 500mL of acidic sodium chlorite solution with the mass fraction of 5%, treating for 5-7h at 80-90 ℃, dissolving out part of components in the wood blocks, enriching micro-nano pore structures of the wood blocks, and forming porous wood blocks; wherein the pH value of the solution is 4, the ratio of the mass of the wood block to the volume of the solution is 1 g:50 mL;
s2, stable pore structure: washing the porous wood block for several times by using deionized water to remove residual chemical agents in the porous wood block; then freeze-drying for 48h at-80 ℃;
s3, amorphous carbon: putting the porous wood block dried in the step S2 into an oven, heating to 200 ℃ and preserving heat for 5 hours, and taking out a sample after cooling; and then putting the sample into a tubular furnace filled with inert protective atmosphere, heating to 750 ℃, preserving heat for 1h, and cooling to obtain the nanoparticle modified porous charcoal containing the three-dimensional amorphous carbon framework.
Example 3
A preparation method of porous charcoal containing a three-dimensional amorphous carbon framework comprises the following steps:
s1, preprocessing: sawing the primary wood (air-dried or oven-dried) into wood blocks with the thickness of 5mm, putting the wood blocks into 500mL of acidic sodium chlorite solution with the mass fraction of 3%, treating for 5-7h at 100 ℃, dissolving out part of components in the wood blocks, enriching micro-nano pore structures of the wood blocks, and forming porous wood blocks; wherein the pH value of the solution is 3, and the ratio of the mass of the wood block to the volume of the solution is 2 g:50 mL;
s2, stable pore structure: washing the porous wood block for several times by using deionized water to remove residual chemical agents in the porous wood block; then freeze-drying for 48h at-50 ℃;
s3, amorphous carbon: putting the porous wood block dried in the step S2 into an oven, heating to 250 ℃, preserving heat for 3 hours, and taking out a sample after cooling; and then putting the sample into a tubular furnace filled with inert protective atmosphere, heating to 700 ℃, preserving heat for 2 hours, and cooling to obtain the nanoparticle modified porous charcoal containing the three-dimensional amorphous carbon framework.
Example 4
A preparation method of porous charcoal containing a three-dimensional amorphous carbon framework comprises the following steps:
s1, preprocessing: sawing the primary wood (air-dried or oven-dried) into wood blocks with the thickness of 10mm, putting the wood blocks into 500mL of mixed solution consisting of sodium hydroxide and sodium sulfite, treating for 5h at 120 ℃, dissolving out part of components in the wood blocks, enriching the micro-nano pore structures of the wood blocks, and forming porous wood blocks; wherein the ratio of the mass of the wood blocks to the volume of the mixed solution is 3g:50 mL;
s2, stable pore structure: repeatedly washing the porous wood block by using deionized water to remove chemical agents remained in the porous wood block; then freeze-drying for 48h at-50 ℃;
s3, amorphous carbon: and (4) putting the porous wood block treated and dried in the step S2 into a tubular furnace filled with inert protective atmosphere, heating to 200 ℃ and preserving heat for 5 hours, and then heating to 600 ℃ and preserving heat for 2 hours to obtain the nanoparticle modified porous charcoal containing the three-dimensional amorphous carbon framework.
Example 5
A preparation method of porous charcoal containing a three-dimensional amorphous carbon framework comprises the following steps:
s1, preprocessing: sawing the primary wood (air-dried or absolutely-dried) into wood blocks with the thickness of 7mm, putting the wood blocks into 500mL of mixed solution of sodium hydroxide and sodium sulfite, treating for 7h at 100 ℃, dissolving out part of components in the wood blocks, enriching micro-nano pore structures of the wood blocks, and forming porous wood blocks; wherein the ratio of the mass of the wood blocks to the volume of the mixed solution is 5g:50 mL;
s2, stable pore structure: washing the porous wood block for several times by using deionized water to remove residual chemical agents in the porous wood block; then freeze-drying for 48h at-50 ℃;
s3, amorphous carbon: and (4) putting the porous wood block dried in the step S2 into a muffle furnace filled with inert protective atmosphere, heating to 250 ℃ and preserving heat for 3h, heating to 650 ℃ and preserving heat for 2.5h, and cooling to obtain the nanoparticle-modified porous charcoal containing the three-dimensional amorphous carbon framework.
Example 6
A preparation method of porous charcoal containing a three-dimensional amorphous carbon framework comprises the following steps:
s1, preprocessing: sawing the primary wood (air-dried or absolutely-dried) into wood blocks with the thickness of 15mm, putting the wood blocks into 500mL of mixed solution of sodium hydroxide and sodium sulfite, treating for 5h at 140 ℃, dissolving out part of components in the wood blocks, enriching micro-nano pore structures of the wood blocks, and forming porous wood blocks; wherein the ratio of the mass of the wood blocks to the volume of the mixed solution is 3g:50 mL;
s2, stable pore structure: washing the porous wood block for several times by using deionized water to remove residual chemical agents in the porous wood block; then freeze-drying for 60h at-80 ℃;
s3, amorphous carbon: and (4) putting the porous wood block dried in the step S2 into a muffle furnace filled with inert protective atmosphere, heating to 300 ℃ and preserving heat for 2h, heating to 750 ℃ and preserving heat for 1h, and cooling to obtain the nanoparticle modified porous charcoal containing the three-dimensional amorphous carbon framework.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. A preparation method of porous charcoal containing a three-dimensional amorphous carbon framework comprises the following steps:
s1, preprocessing: preparing dry wood into a wood block, dissolving out part of components in the wood block through a solvent, and enriching a micro-nano pore structure of the wood block to form a porous wood block;
s2, stable pore structure: washing the porous wood block for several times by using deionized water, and then freeze-drying;
s3, amorphous carbon: and (4) pyrolyzing the porous wood block treated in the step S2 through double temperature gradients to obtain the nanoparticle-modified porous charcoal containing the three-dimensional amorphous carbon framework.
2. The method for preparing porous charcoal containing a three-dimensional amorphous carbon frame according to claim 1, wherein the porous charcoal containing a three-dimensional amorphous carbon frame has a micron-nanometer hierarchical porous structure, a specific surface area of more than 300 square meters per gram and a density of less than 0.25g/cm3。
3. The method for preparing porous charcoal containing three-dimensional amorphous carbon framework according to claim 1, wherein the solvent is an acidic sodium chlorite solution or a mixed solution of sodium hydroxide and sodium sulfite in step S1.
4. The method for preparing porous charcoal containing three-dimensional amorphous carbon framework according to claim 3, wherein the acidic sodium chlorite solution has a mass fraction of 1-10% and a pH value of 2-4; the reaction temperature of the wood blocks in the acidic sodium chlorite solution is 20-100 ℃, and the reaction time is 1-12 h.
5. The method for preparing porous charcoal containing three-dimensional amorphous carbon framework according to claim 4, wherein the ratio of the mass of the wood block to the volume of the acidic sodium chlorite solution is (1-3) g:50 mL.
6. The method for preparing porous charcoal containing a three-dimensional amorphous carbon frame as claimed in claim 3, wherein the reaction temperature of the wood block in the mixed solution is 100-140 ℃ and the reaction time is 3-7 h.
7. The method for preparing porous charcoal containing three-dimensional amorphous carbon framework according to claim 6, wherein the ratio of the mass of the wood piece to the volume of the mixed solution is (1-5) g:50 mL.
8. The method as claimed in claim 1, wherein the pyrolysis step S3 comprises the steps of pyrolysis at a first temperature of 180 ℃ and 300 ℃ for 2-5 h; the second temperature is 500-750 ℃, and the temperature is kept for 1-3 h.
9. A porous charcoal containing a three-dimensional amorphous carbon framework, which is prepared by the method for preparing a porous charcoal containing a three-dimensional amorphous carbon framework according to any one of claims 1 to 8.
10. A wave-absorbing material prepared from the porous charcoal containing the three-dimensional amorphous carbon framework of claim 9.
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